関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Iodine | HCID 807 | — |
| 反応物 | Ammonium cerium-nitrate | HCID 57418452 | — |
| 反応物 | 5-Methoxy-10-oxa-tricyclo[5.2.1.0*2,6*]dec-4-en-3-one | HCID 67283443 | — |
| 溶媒 | Sodium Pyrosulfite | HCID 656671 | — |
| 生成物 | 4-Iodo-5-methoxy-10-oxa-tricyclo[5.2.1.0*2,6*]dec-4-en-3-one | HCID 68569002 | 84.6% |
反応手順
A flask is charged with 5-methoxy-10-oxa-tricyclo[5.2.1.0*2,6*]dec-4-en-3-one (3.96 g, 22 mmol), cerium ammonium nitrate (13.3 g, 24.2 mmol) and iodine (6.73 mg, 26.5 mmol) and then purged with nitrogen. Anhydrous acetonitrile (120 ml) is added, and the reaction heated to 40° C., with stirring for 2 hours. The crude reaction mixture is poured onto a saturated aqueous solution of sodium metabisulphite (250 ml) and extracted with dichloromethane (2×250 ml). The combined organics are dried over magnesium sulphate, filtered, and the solvent is removed under reduced pressure to give 4-Iodo-5-methoxy-10-oxa-tricyclo[5.2.1.0*2,6*]dec-4-en-3-one (5.70 g)
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08530667B2 |
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| 出典データセット | uspto-grants-2013_09 |
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| ORD ID | ord-6e2393f7454c4ffd9ef3a41c6f75f0c0 |
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| 出典メモ | uspto-grants-2013_09 |
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